CN107553074B - Manufacturing method of UNS N08810 iron-nickel based alloy large-caliber seamless pipe for high-temperature heating furnace - Google Patents
Manufacturing method of UNS N08810 iron-nickel based alloy large-caliber seamless pipe for high-temperature heating furnace Download PDFInfo
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Abstract
The manufacturing method of the UNS N08810 iron-nickel based alloy large-caliber seamless pipe for the high-temperature heating furnace comprises the following steps: firstly, directly casting square ingots meeting the requirements by adopting an electric arc smelting method, then cogging the square ingots, then producing a tubular billet by adopting a hot piercing process, and finally controlling the uniform structure of the tubular billet by a cold machining process and a matched heat treatment process and assisting a tubular billet surface treatment process so as to ensure that the tubular billet has high performance and high surface quality. The microstructure of the pipe is isometric crystal, the grain size is 3-5 grade, and the room-temperature tensile property of the finished pipe is as follows: the tensile strength is more than or equal to 500MPa, the yield strength is more than or equal to 210MPa, and the elongation is more than or equal to 50 percent; the tensile properties at 650 ℃ were: the tensile strength is more than or equal to 400MPa, the yield strength is more than or equal to 120MPa, and the elongation is more than or equal to 50%.
Description
Technical Field
The invention belongs to the technical field of iron-nickel base alloy seamless pipe processing, and particularly relates to a method for manufacturing a UNSN08810 iron-nickel base alloy large-caliber seamless pipe for a high-temperature heating furnace.
Background
An iron-nickel based alloy is an alloy between high nickel austenitic stainless steels and nickel based alloys. Compared with nickel-based alloy, the alloy can save nickel by about 40-50 percent, can hold more elements such as chromium, molybdenum and the like in favor of improving the corrosion resistance of the alloy and the content of the elements such as chromium, molybdenum and the like compared with chromium-nickel austenitic stainless steel on the premise of ensuring that an alloy matrix has an austenitic structure with a face-centered cubic structure, and has better thermal stability than the chromium-nickel austenitic stainless steel with high chromium and high molybdenum. In view of the above characteristics of the iron-nickel-based alloy, the iron-nickel-based alloy is widely noticed by chemical processing departments and becomes an alloy with faster development.
The 800 series alloy is a Ni-Cr-Fe system corrosion resistant alloy developed by American Inco-Corporation in 1949, and forms three brands of UNS N08800, UNS N08810 and UNS N08811 by controlling different C, Al and Ti contents, and is respectively applied to different environments. UNS N08810 is developed on the basis of UNS N08800 alloy, and the alloy has good high-temperature mechanical property, higher creep rupture strength, excellent oxidation resistance and certain corrosion resistance, can keep a stable austenite structure when exposed to high temperature for a long time, and has excellent durability; therefore, the UNS N08810 alloy is used in large quantities for the manufacture of catalytic, convective, quench and cracking tubes in the petrochemical industry, radiant tubes, jackets, stills in metallurgical furnaces and high temperature heat exchangers and their fittings in air cooled nuclear reactors.
With the rapid development of the cold hydrogenation technology in the polysilicon industry and the advantages of the UNS N08810 iron-nickel-based alloy, the core equipment high-temperature heating furnace in the cold hydrogenation technology adopts the UNS N08810 iron-nickel-based alloy large-caliber seamless steel pipe to be processed into a large-scale coil for manufacturing. The difficulties in the manufacturing process of UNS N08810 large-caliber seamless tubes (with the diameter range of phi 168 mm-phi 406mm) mainly include the defects of difficult control of heat treatment grain size, high requirement on mechanical property, difficult control of inner and outer surface quality, corrosion caused by acid pickling and the like, and the surface is easy to crack during coil processing.
Chinese patent CN104328324A discloses a process for producing an iron-nickel based alloy tube, but only relates to the processing process of uns n08810 iron-nickel based alloy rough tube and finished tube, does not relate to the previous smelting and tube blank manufacturing method, and does not explicitly describe the control method of the surface quality of the finished tube, and meanwhile, the rough tube is produced by adopting a hot extrusion process. The process needs secondary heating, primary hole expanding and primary hot extrusion, and has long production period, low yield and high energy consumption. The manufacturing method is difficult to manufacture the UNS N08810 seamless pipe with high comprehensive performance requirements, in particular to the pipe required by large-scale coiling of a high-temperature heating furnace of polycrystalline silicon cold hydrogenation core equipment, and the production cost is high.
Chinese patent 201010538426.0 discloses a forged bar hot extrusion and powerful spinning thinning processing large-caliber nickel-based alloy pipe. The process has high manufacturing cost and low production efficiency, is not suitable for industrial production, and is not suitable for producing pipes required by large-scale coils of high-temperature heating furnaces.
Chinese patent 201010538461.6 discloses a method for processing a small-caliber thin-wall nickel-based alloy pipe by a centrifugal casting, hot extrusion and cold rolling or cold drawing method, wherein the structure of a centrifugally cast pipe blank is thick, the quality of the manufactured pipe cannot meet the requirement of high performance, and meanwhile, only the method for processing the small-caliber thin-wall nickel-based alloy pipe is provided, and the hot extrusion cost is high.
Therefore, the method for manufacturing the large-caliber tube made of the iron-nickel base alloy for the high-temperature heating furnace in the full-flow and low-cost manner is needed to manufacture the UNS N08810 iron-nickel base alloy tube with high comprehensive performance requirement, and the requirement of the large-scale coil tube made of the high-temperature heating furnace of the polycrystalline silicon cold hydrogenation core equipment is met.
Disclosure of Invention
The invention aims to provide a method for manufacturing a UNS N08810 iron-nickel based alloy large-diameter seamless pipe for a high-temperature heating furnace, which has the advantages of low manufacturing cost, short manufacturing period and high pipe yield, and the manufactured large-diameter seamless pipe can meet the manufacturing requirements of a large coil pipe for a polycrystalline silicon heating furnace and the requirements of a 600-900 ℃ high-temperature use environment.
In order to achieve the purpose, the technical scheme of the invention is as follows:
the manufacturing method of the UNS N08810 iron-nickel based alloy large-caliber seamless pipe for the high-temperature heating furnace comprises the following steps:
1) smelting and forging
Smelting by adopting an electric arc furnace smelting method, continuously casting a UNS N08810 alloy square ingot, and then forging into an intermediate round pipe blank, wherein the forging deformation amount is controlled to be 40-60%;
the UNS N08810 alloy square ingot comprises the following chemical components in percentage by weight: c: 0.05-0.08%, P is less than or equal to 0.010%, S is less than or equal to 0.010%, Cr: 19.0-23.0%, Ni: 30.0-35.0%, Al: 0.15-0.60%, Ti: 0.15-0.60% of Fe, more than or equal to 39.5%; at least one of Si more than 0 and less than or equal to 0.5 percent, Mn more than 0 and less than or equal to 1.0 percent and Cu more than 0 and less than or equal to 0.75 percent is also contained; and the above elements need to satisfy the following relation at the same time: al and Ti are more than or equal to 0.30 percent and less than or equal to 0.70 percent, and the balance is inevitable impurities;
2) hot piercing of intermediate round tube blank into tube blank
a) Heating the middle round pipe blank to 1150-1180 ℃ and preserving heat;
b) hot-piercing the heated intermediate circular tube blank into a tubular billet on a hot-piercing unit, wherein in the hot-piercing process, the temperature of the intermediate circular tube blank is controlled to be 1150-1180 ℃, the hot-piercing speed is 50-80 mm/s, and the diameter expansion rate is 5-10%;
c) cooling the hot pierced capillary by water, and cooling to room temperature;
d) removing oxide skin of the water-cooled capillary to obtain a capillary without surface defects;
3) processing of finished pipes
a) Cold processing: cold rolling the surface-free hollow billet obtained in the step 2), wherein the deformation of cold rolling passes is controlled to be 30-50%; if the cold rolling passes are more than two times, carrying out solid solution treatment and oxide skin removal between adjacent cold rolling passes, wherein the temperature of the solid solution treatment is 1050-1130 ℃; if the cold rolling pass is one time, directly carrying out subsequent processing;
b) performing solution treatment on the finished pipe, wherein the temperature of the solution treatment is 1180-1200 ℃, and cooling the pipe to room temperature by water;
c) and (5) surface treatment of the finished pipe.
Preferably, in the step 1), the forging process to form the intermediate circular tube blank is as follows: heating a smelted square ingot, forging and deforming the square ingot to an intermediate specification by using a rapid forging press with a deformation amount of 40-60%, then heating, forging the square ingot to a black skin forging rod by using a radial forging machine, and turning and polishing the square ingot to form the intermediate round pipe blank after air cooling.
Preferably, the surface finish Ra of the intermediate round pipe blank obtained in the step 1) is less than or equal to 1.6 mu m.
Preferably, in the step 2), the heating and heat preservation time of the middle round pipe blank is 2-2.5 minutes for the blank with the thickness of each millimeter.
Preferably, in d) of step 2) and a) of step 3), the scale removal method is shot blasting and acid washing.
More preferably, in step 2) d), scale removal is performed by shot blasting and acid washing, and the method includes: firstly, shot blasting is carried out on the inner surface and the outer surface of a capillary, then the capillary is soaked in a mixed aqueous solution of hydrofluoric acid and nitric acid to remove oxide skin, and the soaking time is 10-30 min; in the mixed aqueous solution of hydrofluoric acid and nitric acid, the weight percentage concentration of the hydrofluoric acid is 2-4%, and the weight percentage concentration of the nitric acid is 5-8%.
More preferably, in step 3) a), the method for removing the scale of the pipe after the solution treatment between the cold working passes is as follows: firstly, carrying out shot blasting treatment on a pipe subjected to solution treatment, and then soaking the pipe in a mixed aqueous solution of hydrofluoric acid and nitric acid to quickly remove oxide skin for 10-20 min; in the mixed aqueous solution of hydrofluoric acid and nitric acid, the weight percentage concentration of the hydrofluoric acid is 2-4%, and the weight percentage concentration of the nitric acid is 5-8%.
Preferably, in step 3) c), the surface treatment method of the finished pipe comprises the following steps: firstly, carrying out shot blasting treatment on a finished pipe, and then soaking the finished pipe in a mixed aqueous solution of hydrofluoric acid and nitric acid to quickly remove oxide skin for 10-20 min; in the mixed aqueous solution of hydrofluoric acid and nitric acid, the weight percentage concentration of the hydrofluoric acid is 2-4%, and the weight percentage concentration of the nitric acid is 5-8%.
More preferably, in the d) of step 2), the a) of step 3), and the c) of step 3): (1) shot blasting on the inner wall of the pipe: the shot blasting nozzle adopts a divergent nozzle, the diameter of a steel shot is less than or equal to 0.3mm, the shot blasting pressure is 5.5-6 kg, and the moving speed of the nozzle is 0.6-0.8 m/min; (2) shot blasting outside the pipe: the diameter of the steel shot is less than or equal to 0.3mm, and the moving speed of the spray head is 2.5-10 m/min; (3) the number of shots on the inner wall of the pipe is at least 2 times of the number of shots on the outer wall.
Furthermore, the microstructure of the iron-nickel-based alloy large-caliber seamless pipe manufactured by the invention is isometric crystal, and the grain size is 3-5 grade.
And then, the room temperature tensile property of the iron-nickel base alloy large-caliber seamless pipe is as follows: the tensile strength is more than or equal to 500MPa, the yield strength is more than or equal to 210MPa, and the elongation is more than or equal to 50 percent; the tensile properties at 650 ℃ were: the tensile strength is more than or equal to 400MPa, the yield strength is more than or equal to 120MPa, and the elongation is more than or equal to 50%.
According to the invention, the forging deformation amount of the tube blank in the step 1) is controlled to be 40-60%, so that the complete breakage of a coarse structure of an ingot can be ensured, the structure density and the structure uniformity of the tube blank are improved, and the material plasticity is increased. Simultaneously, the quick forging and radial forging combined forging process is adopted to cogging the square ingot, thereby ensuring the complete crushing of the coarse structure of the square ingot, producing round tube blanks with uniform structure, increasing the plasticity of materials and saving the energy consumption and consumption.
In the step 2), the middle round pipe blank is heated to 1150-1180 ℃ and then perforated, so that the temperature of the pipe blank from the outer surface to the inner surface can be uniform, and the surface quality of the pipe is improved. In order to reduce the generation of finny fur on the inner wall and fine cracks on the outer surface of the pipe in hot perforation, the hot perforation speed is controlled to be 50-80 mm/s and the diameter expansion rate is controlled to be 5-10%.
In the d) of the step 2), when removing the oxide skin, firstly, the inner surface and the outer surface of the pipe are subjected to shot blasting treatment, so that the state of compact oxide skin on the surface of the pipe is changed, and the oxide skin is easy to fall off during the subsequent pickling treatment.
Step 3), controlling the deformation of a cold rolling pass of the pipe in cold machining to be 30-60%: the alloy of the invention has high room temperature strength, severe material work hardening rate tendency and limited cold deformation capability, and needs multi-pass cold working forming. In order to realize the excellent matching of cold forming and structure and size of products and reduce the damage to equipment, the deformation of cold rolling passes of the pipe is required to be controlled to be 30-50%.
In the step 3), solution treatment at 1050-1130 ℃ is carried out between adjacent cold working passes to eliminate cold deformation stress.
And b) performing solid solution treatment on the finished pipe at 1180-1200 ℃ in the step 3), so that the uniformity of the structure can be realized, and the high requirement of heating equipment on the pipe structure performance can be met.
The pipe finished product manufactured by the alloy has high quality requirement on the inner and outer surfaces, and is easy to cause defects during acid cleaning, thereby influencing subsequent equipment processing. The invention adds a shot blasting process on the basis of the traditional pickling process, and simultaneously adjusts the proportion of the pickling solution, so that the surface of the pipe meets the quality requirement.
The microstructure of the finished product pipe (UNS N08810 alloy large-caliber seamless pipe) obtained by the invention is isometric crystal, the grain size is 3-5 grade, and the room-temperature tensile property of the finished product pipe is as follows: the tensile strength is more than or equal to 500MPa, the yield strength is more than or equal to 210MPa, and the elongation is more than or equal to 50 percent; the finished pipe has the tensile property at 650 ℃ as follows: the tensile strength is more than or equal to 400MPa, the yield strength is more than or equal to 120MPa, and the elongation is more than or equal to 50 percent; the alloy pipe has the qualification rate of more than or equal to 98 percent by ultrasonic detection one by one according to the requirement of L2 level in GB/T5777-2008; the inspection qualification rate of the interlayer is 100 percent; the finished pipe has the inner and outer surface smoothness Ra of less than or equal to 3.2 microns and no crack after coiling.
The invention has the beneficial effects that:
1. compared with the traditional manufacturing process for producing the round pipe billet by smelting in an electric arc furnace, electroslag remelting and forging, the manufacturing process for producing the round pipe billet by smelting in the electric arc furnace, continuously casting the square billet and forging reduces the electroslag process, and has short production flow and low manufacturing cost.
2. The invention adopts the hot perforation process to manufacture the large-caliber hollow billet (the diameter range is phi 168 mm-phi 406mm), ensures that the internal structure of the tubular billet is uniform, the wall thickness uniformity and the external diameter roundness are better, the yield is high, and the manufacturing cost is low.
3. The pipe finished product manufactured by the alloy has high quality requirement on the inner and outer surfaces, and the oxide skin on the surface of the pipe is treated by adopting the shot blasting process and the acid pickling process, so that the risk of local over-corrosion on the surface of the pipe is avoided.
4. The method comprises the steps of smelting steel ingots, cogging the steel ingots and controlling the forging deformation amount to be 20-60%, so that the gross structure of the steel ingots is completely crushed, round tube blanks with uniform structures are produced, the material plasticity is increased, and the energy consumption has been saved; then, producing a capillary with uniform tissue by adopting a hot perforation process; and then the cold rolling process, the matched heat treatment process and the surface treatment process are carried out to gradually control the uniform structure and the high surface quality of the pipe, so that the pipe with excellent comprehensive performance is obtained, and the method is particularly suitable for the manufacturing requirement of large-scale coil pipes for polysilicon heating furnaces.
Detailed Description
The technical solution of the present invention is further described in detail with reference to the specific examples below.
Example 1
Specification of
Preparing the UNS N08810 large-caliber pipe.
1) Forging cast ingot into intermediate round pipe blank
Smelting a UNSN08810 alloy square ingot with the following chemical components (in percentage by weight) by adopting an electric arc furnace smelting method:
c: 0.05%, P: 0.005%, S: 0.002%, Si: 0.3%, Mn: 0.5%, Cr: 19.0%, Ni: 30.0%, Cu: 0.50%, Al: 0.15%, Ti: 0.15%, Al + Ti: 0.30 percent, more than or equal to 39.5 percent of Fe and the balance of inevitable impurities.
Size of UNS N08810 alloy ingot: the height × width × length is 200 × 500 × 3000 mm. Heating the smelted square ingot, forging the square ingot to be octagonal by adopting a quick forging press, wherein the deformation is 60%, then, thermally conveying the square ingot to a heating furnace for heating, finally, forging the square ingot to be 241mm black skin forging rod by adopting a radial forging machine, and turning and polishing the square ingot (namely the middle round pipe blank) after air cooling, wherein the surface finish Ra of the blank of the middle round pipe blank is less than or equal to 1.6 mu m.
2) Hot-piercing the intermediate round tube blank into a hollow billet, and performing hot piercing on the hollow billet obtained in the step 1) by using a hot piercing machine according to a hot piercing process of the following steps, wherein the size of the hollow billet subjected to hot piercing is
The steps of hot perforation into the capillary are as follows:
a) cutting the middle circular tube blank into sections, heating to 1150 ℃, and preserving heat for 2 minutes for each millimeter of blank;
b) and (3) hot-piercing the heated intermediate circular tube blank into a tubular billet on a hot-piercing unit, wherein the temperature of the intermediate circular tube blank is 1150 ℃ in the hot-piercing process, the hot-piercing speed is 50mm/s, and the diameter expansion rate is 5.8%.
c) Rapidly cooling the capillary tube subjected to hot perforation by adopting water, and cooling to room temperature;
d) removing oxide skin of the cooled tubular billet to obtain the tubular billet with a defect-free surface: and (3) shot blasting the pipe, and then soaking the pipe in a mixed aqueous solution of hydrofluoric acid and nitric acid to quickly remove oxide skin, wherein the soaking time is 10 min. In the mixed aqueous solution of hydrofluoric acid and nitric acid, the weight percentage concentration of hydrofluoric acid is 2% and the weight percentage concentration of nitric acid is 8%.
The shot blasting treatment is as follows:
shot blasting on the inner wall of the pipe: the spray head adopts a divergent spray head, the diameter of a steel shot is less than or equal to 0.3mm, and the shot blasting pressure is as follows: 5.5kg, the moving speed of the spray head is 0.6 m/min.
Shot blasting on the outer wall of the pipe: the diameter of the steel shot is less than or equal to 0.3mm, and the moving speed of the spray head is 2.5 m/min.
Thirdly, the inner wall of the shot blasting frequency is 2 times of that of the outer wall.
3) Processing of finished pipes
a) Subjecting the surface-defect-free raw pipe obtained in step 2) to 1-pass rolling, i.e. from
Pass deformation amount is 47%;
b) for cold rolling to finished products
Carrying out finished product solution treatment on the steel pipe, wherein the solution temperature is 1180 ℃, and rapidly cooling the steel pipe to room temperature after heat treatment;
c) carrying out surface treatment on the finished pipe after the solution treatment: the pipe after the solution treatment is subjected to shot blasting and then is soaked in a mixed aqueous solution of hydrofluoric acid and nitric acid to rapidly remove oxide skin, and the soaking time is 10 min; in the mixed aqueous solution of hydrofluoric acid and nitric acid, the weight percentage concentration of hydrofluoric acid is 2% and the weight percentage concentration of nitric acid is 5%.
The shot blasting treatment is as follows:
shot blasting on the inner wall of the pipe: the spray head adopts a divergent spray head, the diameter of a steel shot is less than or equal to 0.3mm, and the shot blasting pressure is as follows: 5.5kg, the moving speed of the spray head is 0.6 m/min.
Shot blasting on the outer wall of the pipe: the diameter of the steel shot is less than or equal to 0.3mm, and the moving speed of the spray head is 2.5 m/min.
Thirdly, the inner wall of the shot blasting frequency is 2 times of that of the outer wall.
4) Inspection of finished product
The microstructure of the finished pipe is equiaxed crystal, the grain size is 3 grades, and the room-temperature tensile property of the finished pipe is as follows: tensile strength of 540MPa, yield strength of 220MPa and elongation of 55 percent; the tensile property of the finished pipe at 650 ℃ is as follows: tensile strength of 450MPa, yield strength of 140MPa and elongation of 60 percent; the alloy pipe has the qualification rate of more than or equal to 98 percent by ultrasonic detection one by one according to the requirement of L2 level in GB/T5777-2008; the inspection qualification rate of the interlayer is 100 percent; inner and outer surface finishment Ra of finished pipe: 3.0 μm, no cracking after coiling, and meeting the manufacturing requirements of large-scale coils for polysilicon heating furnaces.
Example 2
Specification of
Preparing the UNS N08810 large-caliber pipe.
1) Forging cast ingot into intermediate round pipe blank
Smelting a UNSN08810 alloy square ingot with the following chemical components (in percentage by weight) by adopting an electric arc furnace smelting method:
c: 0.05%, P: 0.005%, S: 0.002%, Si: 0.2%, Mn: 0.5%, Cr: 19.0%, Ni: 30.0%, Cu: 0.20%, Al: 0.15%, Ti: 0.15%, Al + Ti: 0.30 percent, more than or equal to 39.5 percent of Fe and the balance of inevitable impurities.
Size of UNS N08810 alloy ingot: the height × width × length is 200 × 500 × 3000 mm. Heating the smelted square ingot, forging the square ingot to be octagonal by adopting a quick forging press, wherein the deformation is 60%, then, thermally conveying the square ingot to a heating furnace for heating, finally, forging the square ingot to be 241mm black skin forging rod by adopting a radial forging machine, and turning and polishing the square ingot (namely the middle round pipe blank) after air cooling, wherein the surface finish Ra of the blank of the middle round pipe blank is less than or equal to 1.6 mu m.
2) Hot piercing of intermediate round tube blank into tube blank
By the use of heatPerforming tubular billet hot perforation on the smooth blank obtained in the step 1) by a perforating machine according to a hot perforation process of the following steps, wherein the tubular billet of the hot perforation has the size of
The steps of hot perforation into the capillary are as follows:
a) cutting the obtained intermediate circular tube blank into sections, heating to 1180 ℃, and preserving heat for 2.5 minutes for each millimeter of blank;
b) hot piercing the heated intermediate circular tube blank into a tubular billet on a hot piercing unit, wherein the temperature of the intermediate circular tube blank is 1180 ℃ in the hot piercing process, the hot piercing speed is 80mm/s, and the diameter expansion rate is 5.8%;
c) rapidly cooling the capillary tube subjected to hot perforation by adopting water;
d) removing oxide skin of the cooled tubular billet to obtain a tubular billet with a defect-free surface; and (3) shot blasting the pipe, and then soaking the pipe in a mixed aqueous solution of hydrofluoric acid and nitric acid to quickly remove oxide skin, wherein the soaking time is 20 min. In the mixed aqueous solution of hydrofluoric acid and nitric acid, the weight percentage concentration of hydrofluoric acid is 4% and the weight percentage concentration of nitric acid is 5%.
The shot blasting treatment is as follows:
shot blasting on the inner wall of the pipe: the spray head adopts a divergent spray head, the diameter of a steel shot is less than or equal to 0.3mm, and the shot blasting pressure is as follows: 6.0kg, the moving speed of the spray head is 0.8 m/min.
Shot blasting on the outer wall of the pipe: the diameter of the steel shot is less than or equal to 0.3mm, and the moving speed of the spray head is 10 m/min.
Thirdly, the inner wall of the shot blasting frequency is 2 times of that of the outer wall.
3) Processing of finished pipes
a) Performing 2-pass rolling on the surface-defect-free hollow billet obtained in the step 2) until
Pass deformation is 40%;
b) 2-time solution treatment of cold working: the solid solution temperature is 1100 ℃, when the oxide skin is removed after the solid solution treatment, the pipe is shot-blasted and then is soaked in a mixed aqueous solution of hydrofluoric acid and nitric acid to rapidly remove the oxide skin, and the soaking time is 20 min. In the mixed aqueous solution of hydrofluoric acid and nitric acid, the weight percentage concentration of hydrofluoric acid is 4% and the weight percentage concentration of nitric acid is 8%.
The shot blasting treatment is as follows:
shot blasting on the inner wall of the pipe: the spray head adopts a divergent spray head, the diameter of a steel shot is less than or equal to 0.3mm, and the shot blasting pressure is as follows: 6.0kg, the moving speed of the spray head is 0.8 m/min.
Shot blasting on the outer wall of the pipe: the diameter of the steel shot is less than or equal to 0.3mm, and the moving speed of the spray head is 10 m/min.
Thirdly, the inner wall of the shot blasting frequency is 2 times of that of the outer wall.
c) For cold rolling to finished products
Carrying out finished product solution treatment on the steel pipe, wherein the solution temperature is 1200 ℃, and rapidly cooling the steel pipe to room temperature after heat treatment;
d) and carrying out surface treatment on the finished pipe after the solution heat treatment. And (3) shot blasting the pipe, and then soaking the pipe in a mixed aqueous solution of hydrofluoric acid and nitric acid to quickly remove oxide skin, wherein the soaking time is 15 min. In the mixed aqueous solution of hydrofluoric acid and nitric acid, the weight percentage concentration of hydrofluoric acid is 3% and the weight percentage concentration of nitric acid is 7%.
The shot blasting treatment is as follows:
shot blasting on the inner wall of the pipe: the spray head adopts a divergent spray head, the diameter of a steel shot is less than or equal to 0.3mm, and the shot blasting pressure is as follows: 6.0kg, the moving speed of the spray head is 0.8 m/min.
Shot blasting on the outer wall of the pipe: the diameter of the steel shot is less than or equal to 0.3mm, and the moving speed of the spray head is 10 m/min.
Thirdly, the inner wall of the shot blasting frequency is 2 times of that of the outer wall.
4) Inspection of finished product
The microstructure of the finished pipe is equiaxed crystal, the grain size is 4.5 grade, and the room-temperature tensile property of the finished pipe is as follows: tensile strength is 550MPa, yield strength is 230MPa, and elongation is 55%; the tensile property of the finished pipe at 650 ℃ is as follows: the tensile strength is 460MPa, the yield strength is 145MPa, and the elongation is 58%; the alloy pipe has the qualification rate of 100 percent by ultrasonic detection one by one according to the requirement of L2 grade in GB/T5777-2008; the inspection qualification rate of the interlayer is 100 percent; inner and outer surface finishment Ra of finished pipe: 3.0 μm, no cracking after coiling, and meeting the manufacturing requirements of large-scale coils for polysilicon heating furnaces.
Example 3
Specification of
Preparing the UNS N08810 large-caliber pipe.
1) Forging cast ingot into intermediate round pipe blank
Smelting a UNSN08810 alloy square ingot with the following chemical components (in percentage by weight) by adopting an electric arc furnace smelting method:
c: 0.05%, P: 0.005%, S: 0.002%, Si: 0.3%, Mn: 0.4%, Cr: 19.0%, Ni: 30.0%, Cu: 0.30%, Al: 0.15%, Ti: 0.15%, Al + Ti: 0.30 percent, more than or equal to 39.5 percent of Fe and the balance of inevitable impurities.
The size of the UNS N08810 alloy ingot is that the height ×, the width × and the length are 200 × 500 × 3000mm, the smelted square ingot is heated, then a quick forging press is adopted to forge the square ingot to an octagon with the deformation of 40 percent, then the square ingot is heated in a heating furnace, and finally a radial forging machine is adopted to forge the square ingot to the shape of a square ingot
And (3) forging the rod with black skin, and polishing (namely the middle round pipe blank) after air cooling, wherein the blank surface finish Ra of the middle round pipe blank is less than or equal to 1.6 mu m.
2) Hot piercing of intermediate round tube blank into tube blank
Performing tubular billet hot perforation on the smooth blank obtained in the step 1) by using a hot perforating machine according to a hot perforation process of the following steps, wherein the tubular billet of the hot perforation has the size of
The steps of hot perforation into the capillary are as follows:
a) cutting the obtained intermediate circular tube blank into sections, heating to 1180 ℃, and preserving heat for 2.5 minutes for each millimeter of blank;
b) hot piercing the heated intermediate circular tube blank into a tubular billet on a hot piercing unit, wherein the temperature of the intermediate circular tube blank is 1160 ℃, the hot piercing speed is 60mm/s, and the diameter expansion rate is 9.0 percent in the hot piercing process;
c) rapidly cooling the capillary tube subjected to hot perforation by adopting water;
d) removing oxide skin of the cooled tubular billet to obtain a tubular billet with a defect-free surface; and (3) shot blasting the pipe, and then soaking the pipe in a mixed aqueous solution of hydrofluoric acid and nitric acid to quickly remove oxide skin, wherein the soaking time is 15 min. In the mixed aqueous solution of hydrofluoric acid and nitric acid, the weight percentage concentration of hydrofluoric acid is 3% and the weight percentage concentration of nitric acid is 7%.
The shot blasting treatment is as follows:
shot blasting on the inner wall of the pipe: the spray head adopts a divergent spray head, the diameter of a steel shot is less than or equal to 0.3mm, and the shot blasting pressure is as follows: 6.0kg, the moving speed of the spray head is 0.8 m/min.
Shot blasting on the outer wall of the pipe: the diameter of the steel shot is less than or equal to 0.3mm, and the moving speed of the spray head is 8 m/min.
Thirdly, the inner wall of the shot blasting frequency is 2 times of that of the outer wall.
3) Processing of finished pipes
a) Performing 1-pass rolling on the surface-defect-free hollow billet obtained in the step 2) to obtain
Pass deformation is 46%;
b) for cold rolling to finished products
Carrying out finished product solution treatment on the steel pipe, wherein the solution temperature is 1180 ℃, and rapidly cooling the steel pipe to room temperature after heat treatment;
c) and carrying out surface treatment on the finished pipe subjected to the solution treatment. And (3) shot blasting the pipe, and then soaking the pipe in a mixed aqueous solution of hydrofluoric acid and nitric acid to quickly remove oxide skin, wherein the soaking time is 15 min. In the mixed aqueous solution of hydrofluoric acid and nitric acid, the weight percentage concentration of hydrofluoric acid is 3% and the weight percentage concentration of nitric acid is 7%.
The shot blasting treatment is as follows:
shot blasting on the inner wall of the pipe: the spray head adopts a divergent spray head, the diameter of a steel shot is less than or equal to 0.3mm, and the shot blasting pressure is as follows: 6.0kg, the moving speed of the spray head is 0.8 m/min.
Shot blasting on the outer wall of the pipe: the diameter of the steel shot is less than or equal to 0.3mm, and the moving speed of the spray head is 10 m/min.
Thirdly, the inner wall of the shot blasting frequency is 2 times of that of the outer wall.
4) Inspection of finished product
The microstructure of the finished pipe is equiaxed crystal, the grain size is 3 grades, and the room-temperature tensile property of the finished pipe is as follows: tensile strength is 550MPa, yield strength is 230MPa, and elongation is 57%; the tensile property of the finished pipe at 650 ℃ is as follows: tensile strength of 450MPa, yield strength of 140MPa and elongation of 60 percent; the alloy pipe has the qualification rate of more than or equal to 98 percent by ultrasonic detection one by one according to the requirement of L2 level in GB/T5777-2008; the inspection qualification rate of the interlayer is 100 percent; inner and outer surface finishment Ra of finished pipe: 3.0 μm, no cracking after coiling, and meeting the manufacturing requirements of large-scale coils for polysilicon heating furnaces.
Example 4
Specification of
Preparing the UNS N08810 large-caliber pipe.
1) Forging cast ingot into intermediate round pipe blank
Smelting a UNSN08810 alloy square ingot with the following chemical components (in percentage by weight) by adopting an electric arc furnace smelting method:
c: 0.07%, P: 0.005%, S: 0.002%, Si: 0.5%, Mn: 0.7%, Cr: 21.0%, Ni: 32.0%, Cu: 0.50%, Al: 0.20%, Ti: 0.25%, Al + Ti: 0.45 percent, more than or equal to 39.5 percent of Fe and the balance of inevitable impurities.
Heating the smelted square ingot, forging to an octagonal shape by adopting a quick forging press with the deformation amount of 20%, then heating to a heating furnace, and finally forging to an octagonal shape by adopting a radial forging machine
And (3) forging the rod with black skin, and polishing (namely the middle round pipe blank) after air cooling, wherein the blank surface finish Ra of the middle round pipe blank is less than or equal to 1.6 mu m.
2) Hot piercing of intermediate round tube blank into tube blank
Performing tubular billet hot perforation on the smooth blank obtained in the step 1) by using a hot perforating machine according to a hot perforation process of the following steps, wherein the tubular billet of the hot perforation has the size of
The steps of hot perforation into the capillary are as follows:
a) cutting the obtained intermediate circular tube blank into sections, heating to 1180 ℃, and preserving heat for 2.5 minutes for each millimeter of blank;
b) hot piercing the heated intermediate round pipe blank into a tubular billet on a hot piercing unit, wherein the temperature of the intermediate round pipe blank is 1170 ℃, the hot piercing speed is 60mm/s, and the diameter expansion rate is 9.5 percent in the hot piercing process;
c) rapidly cooling the capillary tube subjected to hot perforation by adopting water;
d) removing oxide skin of the cooled tubular billet to obtain a tubular billet with a defect-free surface; and (3) shot blasting the pipe, and then soaking the pipe in a mixed aqueous solution of hydrofluoric acid and nitric acid to quickly remove oxide skin, wherein the soaking time is 15 min. In the mixed aqueous solution of hydrofluoric acid and nitric acid, the weight percentage concentration of hydrofluoric acid is 3% and the weight percentage concentration of nitric acid is 7%.
The shot blasting treatment is as follows:
shot blasting on the inner wall of the pipe: the spray head adopts a divergent spray head, the diameter of a steel shot is less than or equal to 0.3mm, and the shot blasting pressure is as follows: 6.0kg, the moving speed of the spray head is 0.8 m/min.
Shot blasting on the outer wall of the pipe: the diameter of the steel shot is less than or equal to 0.3mm, and the moving speed of the spray head is 8 m/min.
Thirdly, the inner wall of the shot blasting frequency is 2 times of that of the outer wall.
3) Processing of finished pipes
a) Performing 1-pass rolling on the surface-defect-free hollow billet obtained in the step 2) to obtain
Pass deformation is 45.8%;
b) for cold rolling to finished products
Carrying out finished product solution treatment on the steel pipe, wherein the solution temperature is 1180 ℃, and rapidly cooling the steel pipe to room temperature after heat treatment;
c) and carrying out surface treatment on the finished pipe subjected to the solution treatment. And (3) shot blasting the pipe, and then soaking the pipe in a mixed aqueous solution of hydrofluoric acid and nitric acid to quickly remove oxide skin, wherein the soaking time is 15 min. In the mixed aqueous solution of hydrofluoric acid and nitric acid, the weight percentage concentration of hydrofluoric acid is 3% and the weight percentage concentration of nitric acid is 7%.
The shot blasting treatment is as follows:
shot blasting on the inner wall of the pipe: the spray head adopts a divergent spray head, the diameter of a steel shot is less than or equal to 0.3mm, and the shot blasting pressure is as follows: 6.0kg, the moving speed of the spray head is 0.8 m/min.
Shot blasting on the outer wall of the pipe: the diameter of the steel shot is less than or equal to 0.3mm, and the moving speed of the spray head is 8 m/min.
Thirdly, the inner wall of the shot blasting frequency is 2 times of that of the outer wall.
4) Inspection of finished product
The microstructure of the finished pipe is equiaxed crystal, the grain size is 3 grades, and the room-temperature tensile property of the finished pipe is as follows: tensile strength is 550MPa, yield strength is 230MPa, and elongation is 57%; the tensile property of the finished pipe at 650 ℃ is as follows: tensile strength of 450MPa, yield strength of 140MPa and elongation of 60 percent; the alloy pipe has the qualification rate of more than or equal to 98 percent by ultrasonic detection one by one according to the requirement of L2 level in GB/T5777-2008; the inspection qualification rate of the interlayer is 100 percent; inner and outer surface finishment Ra of finished pipe: 3.0 μm, no cracking after coiling, and meeting the manufacturing requirements of large-scale coils for polysilicon heating furnaces.
The above embodiments describe the features of the present invention in more detail, but the invention is not limited thereto, and other changes and modifications may be made without departing from the spirit of the invention, and the changes and modifications fall within the scope of the invention.
Claims (11)
1. The manufacturing method of the UNS N08810 iron-nickel based alloy large-caliber seamless pipe for the high-temperature heating furnace comprises the following steps:
1) smelting and forging:
smelting and continuously casting a UNS N08810 alloy square ingot by adopting an electric arc furnace smelting method, and then forging the square ingot into an intermediate round pipe blank, wherein the forging deformation is controlled to be 40-60%;
the UNS N08810 alloy square ingot comprises the following chemical components in percentage by weight: c: 0.05-0.08%, P is less than or equal to 0.010%, S is less than or equal to 0.010%, Cr: 19.0-23.0%, Ni: 30.0-35.0%, Al: 0.15-0.60%, Ti: 0.15-0.60% of Fe, more than or equal to 39.5%; at least one of Si more than 0 and less than or equal to 0.5 percent, Mn more than 0 and less than or equal to 1.0 percent and Cu more than 0 and less than or equal to 0.75 percent is also contained; and Al and Ti need to satisfy the following relational expressions simultaneously: al and Ti are more than or equal to 0.30 percent and less than or equal to 0.70 percent, and the balance is inevitable impurities;
2) hot piercing of intermediate round tube blank into tube blank
a) Heating the middle round pipe blank to 1150-1180 ℃ and preserving heat;
b) hot piercing the heated middle round tube blank into a tubular billet, wherein in the hot piercing process, the temperature of the middle round tube blank is controlled to be 1150-1180 ℃, the hot piercing speed is 50-80 mm/s, and the diameter expansion rate is 5-10%;
c) cooling the hot pierced capillary to room temperature;
d) removing oxide skin of the water-cooled capillary to obtain a capillary without surface defects;
3) processing of finished pipes
a) Cold processing: cold rolling the surface-free hollow billet obtained in the step 2), wherein the deformation amount of each cold rolling pass is controlled to be 30-50%; if the cold rolling passes are more than two times, performing solid solution treatment and oxide skin removal between adjacent cold rolling passes, wherein the temperature of the solid solution treatment is 1050-1130 ℃; if the cold rolling pass is one time, directly carrying out subsequent processing;
b) solution treatment of the finished pipe: the temperature of the solution treatment is 1180-1200 ℃, and the solution treatment is carried out by water cooling to room temperature;
c) surface treatment of the finished pipe;
the microstructure of the iron-nickel base alloy UNS N08810 large-caliber pipe is isometric crystal, the grain size is 3-5 grade, and the room-temperature tensile property is as follows: the tensile strength is more than or equal to 500MPa, the yield strength is more than or equal to 210MPa, and the elongation is more than or equal to 50 percent; the tensile properties at 650 ℃ were: the tensile strength is more than or equal to 400MPa, the yield strength is more than or equal to 120MPa, and the elongation is more than or equal to 50%.
2. The method for manufacturing UNS N08810 iron-nickel based alloy large-caliber seamless tube material for the high-temperature heating furnace according to claim 1, wherein in the step 1), the forging process to form the intermediate circular tube blank is as follows: heating a square ingot, forging the square ingot by a rapid forging press until the deformation amount of the square ingot is 40-60%, forging the square ingot to an intermediate specification, then heating the square ingot, forging the square ingot to a black skin forged rod by a radial forging machine, and turning the square ingot into the intermediate round pipe blank after air cooling.
3. The method for manufacturing UNS N08810 iron-nickel based alloy large-caliber seamless pipe material for the high-temperature heating furnace according to claim 1 or 2, characterized in that the surface finish Ra of the intermediate round pipe blank obtained in the step 1) is less than or equal to 1.6 μm.
4. The method for manufacturing UNS N08810 iron-nickel based alloy large-caliber seamless pipe material for the high-temperature heating furnace according to claim 1, wherein in the step 2), the heating and heat preservation time of the intermediate circular pipe blank is 2-2.5 minutes for preserving the heat of the blank with the thickness of each millimeter.
5. The method for manufacturing UNS N08810 iron-nickel based alloy large-diameter seamless pipe material for a high-temperature heating furnace according to claim 1, wherein the scale removal method in step 2) d) and step 3) a) is shot blasting and acid pickling.
6. The method for manufacturing UNS N08810 iron-nickel based alloy large-diameter seamless pipe material for the high-temperature heating furnace according to claim 1 or 5, wherein in step 2) d), the scale is removed as follows: firstly, shot blasting is carried out on the inner surface and the outer surface of a capillary, then the capillary is soaked in a mixed aqueous solution of hydrofluoric acid and nitric acid to quickly remove oxide skin, and the soaking time is 10-30 min; in the mixed aqueous solution of hydrofluoric acid and nitric acid, the weight percentage concentration of the hydrofluoric acid is 2-4%, and the weight percentage concentration of the nitric acid is 5-8%.
7. The method for manufacturing UNS N08810 iron-nickel based alloy large-diameter seamless pipe material for the high-temperature heating furnace according to claim 1 or 5, wherein in the step a) of step 3), the method for removing the oxide skin of the pipe material after the solution treatment between the adjacent cold working passes is as follows: firstly, carrying out shot blasting treatment on a pipe subjected to solution treatment, and then soaking the pipe in a mixed aqueous solution of hydrofluoric acid and nitric acid to quickly remove oxide skin for 10-20 min; the weight percentage concentration of hydrofluoric acid in the mixed aqueous solution of hydrofluoric acid and nitric acid is 2-4%, and the weight percentage concentration of nitric acid is 5-8%.
8. The method for manufacturing UNS N08810 iron-nickel based alloy large-caliber seamless pipe material for the high-temperature heating furnace according to claim 1, wherein in the step c) of step 3), the surface treatment of the finished pipe material is as follows: firstly, carrying out shot blasting treatment on a finished pipe, and then soaking the finished pipe in a mixed aqueous solution of hydrofluoric acid and nitric acid to remove oxide skin for 10-20 min; in the mixed aqueous solution of hydrofluoric acid and nitric acid, the weight percentage concentration of the hydrofluoric acid is 2-4%, and the weight percentage concentration of the nitric acid is 5-8%.
9. The method for manufacturing UNS N08810 iron-nickel based alloy large-diameter seamless pipe material for high-temperature heating furnace according to claim 5 or 8, wherein in the shot blasting process: (1) shot blasting on the inner wall of the pipe: the shot blasting nozzle adopts a divergent nozzle, the diameter of a steel shot is less than or equal to 0.3mm, the shot blasting pressure is 5.5-6 kg, and the moving speed of the nozzle is 0.6-0.8 m/min; (2) shot blasting on the outer wall of the pipe: the diameter of the steel shot is less than or equal to 0.3mm, and the moving speed of the spray head is 2.5-10 m/min; (3) the shot blasting frequency of the inner wall of the pipe is more than 2 times of the shot blasting frequency of the outer wall.
10. The method for manufacturing UNS N08810 iron-nickel based alloy large-diameter seamless pipe material for the high-temperature heating furnace according to claim 6, wherein in the shot blasting process: (1) shot blasting on the inner wall of the pipe: the shot blasting nozzle adopts a divergent nozzle, the diameter of a steel shot is less than or equal to 0.3mm, the shot blasting pressure is 5.5-6 kg, and the moving speed of the nozzle is 0.6-0.8 m/min; (2) shot blasting on the outer wall of the pipe: the diameter of the steel shot is less than or equal to 0.3mm, and the moving speed of the spray head is 2.5-10 m/min; (3) the shot blasting frequency of the inner wall of the pipe is more than 2 times of the shot blasting frequency of the outer wall.
11. The method for manufacturing UNS N08810 iron-nickel based alloy large-diameter seamless pipe material for the high-temperature heating furnace according to claim 7, wherein in the shot blasting process: (1) shot blasting on the inner wall of the pipe: the shot blasting nozzle adopts a divergent nozzle, the diameter of a steel shot is less than or equal to 0.3mm, the shot blasting pressure is 5.5-6 kg, and the moving speed of the nozzle is 0.6-0.8 m/min; (2) shot blasting on the outer wall of the pipe: the diameter of the steel shot is less than or equal to 0.3mm, and the moving speed of the spray head is 2.5-10 m/min; (3) the shot blasting frequency of the inner wall of the pipe is more than 2 times of the shot blasting frequency of the outer wall.
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| CN111618095A (en) * | 2020-06-12 | 2020-09-04 | 攀钢集团江油长城特殊钢有限公司 | Preparation method of UNS N06690 nickel-based alloy pierced billet |
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